CN102557297B - Treatment method of waste liquid after cleaning copper plated layer of printed circuit board - Google Patents
Treatment method of waste liquid after cleaning copper plated layer of printed circuit board Download PDFInfo
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- CN102557297B CN102557297B CN2011104578055A CN201110457805A CN102557297B CN 102557297 B CN102557297 B CN 102557297B CN 2011104578055 A CN2011104578055 A CN 2011104578055A CN 201110457805 A CN201110457805 A CN 201110457805A CN 102557297 B CN102557297 B CN 102557297B
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- copper
- waste liquid
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- zinc
- copper powder
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a treatment method of waste liquid after cleaning a copper plated layer of a printed circuit board. The treatment method comprises the following steps: adding zinc powder of 50-80 meshes and percentage by weight of 99.9% into the waste liquid obtained after cleaning the copper plated layer of the printed circuit board for reaction, wherein the adding amount of the zinc powder is 260-310g per liter of the waste liquid and the reaction temperature is 70-80 DEG C; performing electromagnetic stirring reaction for 4-4.5 hours while adding the zinc powder to get a zinc chloride solution and copper powder; driving the solution after the reaction into a settling tank for settling for 20-24 hours, performing precipitation separation on supernatant fluid of zinc chloride from copper powder at the bottom layer, performing evaporation and crystallization on the supernatant fluid to obtain anhydrous zinc dichloride, filtering and washing the copper powder separated by precipitation, and drying for 20-24 hours at the temperature of 120-150 DEG C under the protection of inert gas to obtain a copper powder product. The anhydrous zinc dichloride obtained by adopting the treatment method disclosed by the invention is tested to completely conform to indexes of industrial stage II anhydrous zinc dichloride; and the copper amount in the obtained copper powder is not less than 98%, and the process is simple and significant in recovery value.
Description
Technical field
The present invention relates to a kind for the treatment of process of contained waste liquid, be specifically related to the treatment process of in a kind of printed circuit board (PCB) preparation residual copper coating being cleaned the waste liquid that produces.
Background technology
Copper layer composite panel of plastic material is the starting material of printed wiring circuit board, and copper coating unnecessary in preparation process is cleaned, and remaining copper coating and plastic plate namely form the desired printed wiring circuit board of design.Contain a large amount of metallic copper compositions in the keto-acid containing waste liquid that copper coating after the cleaning produces, should accomplish economy, reclaim valuable metal copper effectively, again environment not being had any discharging that exceeds standard is present technological difficulties.
Residual copper coating adopts hydrochloric acid to clean the about 122.53g/l of copper ions in the waste liquid that produces in the preparation of printed wiring circuit board, the about 266.06g/L of chloride ion-containing, contain the about 0.83g/L of ferrous ion, this contained waste liquid corrodibility is very strong, extremely strong titanium plate, the stainless steel of erosion resistance all suffers heavy corrosion and can not use in conventional electrodeposition method, therefore must find to overcome the unconventional technology that chlorion corrodes, can extract metallic copper again, this does not see any related data at home and abroad.
Summary of the invention
The object of the invention is to provide a kind of economy, handles the method for the waste liquid after the printed circuit board (PCB) copper coating cleans efficiently.
The object of the invention realizes by following technique means:
The treatment process of the waste liquid after a kind of printed circuit board (PCB) copper coating cleans, it is characterized in that: be that 99.9% zinc powder adds in the waste liquid after the printed circuit board (PCB) copper coating cleans and reacts with 50～80 orders, weight percentage, the zinc powder add-on is that every liter of waste liquid adds 260～310g, temperature of reaction is 70～80 ℃, and the limit adds the induction stirring reaction of zinc powder limit and obtained liquor zinci chloridi and copper powder in 4～4.5 hours; Reacted solution was squeezed into settling pool heavy clear 20～24 hours; supernatant liquor zinc chloride and bottom copper powder precipitate and separate, supernatant liquor evaporative crystallization are obtained anhydrous zinc dichloride; the copper powder of described precipitate and separate is filtered, washs, and 120～150 ℃ of oven dry obtained the copper powder product in 20～24 hours under protection of inert gas again.
The contriver finds in R﹠D process, in the contained waste liquid that is rich in cupric chloride and hydrochloric acid, add zinc powder, though obtain liquor zinci chloridi and copper powder, control not high, the recycling value of the bad liquor zinci chloridi purity that obtains, the copper powder copper content that makes does not reach desirable requirement; The present invention has adopted specific reaction conditions, copper powder has been carried out anti-oxidation oven dry handled, and makes the zinc chloride and the copper powder that make meet utility value fully.
Preferably, the treatment process of the waste liquid after a kind of printed circuit board (PCB) copper coating cleans, it is characterized in that: be that 99.9% zinc powder adds in the waste liquid after the printed circuit board (PCB) copper coating cleans and reacts with 65～80 orders, weight percentage, the zinc powder add-on is that every liter of waste liquid adds 300g, temperature of reaction is 70～75 ℃, and the limit adds the induction stirring reaction of zinc powder limit and obtained liquor zinci chloridi and copper powder in 4 hours; Reacted solution was squeezed into settling pool heavy clear 24 hours; supernatant liquor zinc chloride and bottom copper powder precipitate and separate, supernatant liquor evaporative crystallization are obtained anhydrous zinc dichloride; the copper powder of described precipitate and separate is filtered, washs, and 135 ℃ of oven dry obtained the copper powder product in 22 hours under protection of inert gas again.
The present invention has following beneficial effect:
The anhydrous zinc dichloride that adopts treatment process of the present invention to obtain meets the index of the anhydrous zinc dichloride of industrial secondary after testing fully, and price is about 10000 yuan/t; Copper powder copper content 〉=98% that obtains, market price are 55000-60000 unit/t, and by about 15500 yuan/t of this technology of existing market valency copper powder wound net income per ton, technology is simple, recovery value is remarkable.
Embodiment
Carry out concrete description below by the present invention of embodiment; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, those skilled in the art can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
Embodiment 1
The treatment process of the waste liquid after a kind of printed circuit board (PCB) copper coating cleans, be that 99.9% zinc powder adds in the waste liquid after the printed circuit board (PCB) copper coating cleans and reacts with 65～80 orders, weight percentage, the zinc powder add-on is that every liter of waste liquid adds 300g, temperature of reaction is 75～78 ℃, and the limit adds the induction stirring reaction of zinc powder limit and obtained liquor zinci chloridi and copper powder in 4 hours; Reacted solution was squeezed into settling pool heavy clear 24 hours; supernatant liquor zinc chloride and bottom copper powder precipitate and separate, supernatant liquor evaporative crystallization are obtained anhydrous zinc dichloride; the copper powder of described precipitate and separate is filtered, washs, and 135 ℃ of oven dry obtained the copper powder product in 22 hours under protection of inert gas again.The index that meets the anhydrous zinc dichloride of industrial secondary fully, the copper powder copper content that obtains is 99.5%.
Embodiment 2
The treatment process of the waste liquid after a kind of printed circuit board (PCB) copper coating cleans, be that 99.9% zinc powder adds in the waste liquid after the printed circuit board (PCB) copper coating cleans and reacts with 50～60 orders, weight percentage, the zinc powder add-on is that every liter of waste liquid adds 260g, temperature of reaction is 70～72 ℃, and the limit adds the induction stirring reaction of zinc powder limit and obtained liquor zinci chloridi and copper powder in 4.5 hours; Reacted solution was squeezed into settling pool heavy clear 20 hours; supernatant liquor zinc chloride and bottom copper powder precipitate and separate, supernatant liquor evaporative crystallization are obtained anhydrous zinc dichloride; the copper powder of described precipitate and separate is filtered, washs, and 150 ℃ of oven dry obtained the copper powder product in 24 hours under protection of inert gas again.The index that meets the anhydrous zinc dichloride of industrial secondary fully, the copper powder copper content that obtains is 99.3%.
Embodiment 3
The treatment process of the waste liquid after a kind of printed circuit board (PCB) copper coating cleans, be that 99.9% zinc powder adds in the waste liquid after the printed circuit board (PCB) copper coating cleans and reacts with 60～70 orders, weight percentage, the zinc powder add-on is that every liter of waste liquid adds 280g, temperature of reaction is 78～80 ℃, and the limit adds the induction stirring reaction of zinc powder limit and obtained liquor zinci chloridi and copper powder in 4.5 hours; Reacted solution was squeezed into settling pool heavy clear 22 hours; supernatant liquor zinc chloride and bottom copper powder precipitate and separate, supernatant liquor evaporative crystallization are obtained anhydrous zinc dichloride; the copper powder of described precipitate and separate is filtered, washs, and 120 ℃ of oven dry obtained the copper powder product in 20 hours under protection of inert gas again.The index that meets the anhydrous zinc dichloride of industrial secondary fully, the copper powder copper content that obtains is 99.0%.
Claims (2)
1. the treatment process of the waste liquid after a printed circuit board (PCB) copper coating cleans, it is characterized in that: be that 99.9% zinc powder adds in the waste liquid after the printed circuit board (PCB) copper coating cleans and reacts with 50 ~ 80 orders, weight percentage, adding the zinc powder amount is that every liter of waste liquid adds 260 ~ 310g, temperature of reaction is 70 ~ 78 ℃, and the limit adds the induction stirring reaction of zinc powder limit and obtained liquor zinci chloridi and copper powder in 4 ~ 4.5 hours; Reacted solution was squeezed into settling pool heavy clear 20 ~ 24 hours; supernatant liquor zinc chloride and bottom copper powder precipitate and separate, supernatant liquor evaporative crystallization are obtained anhydrous zinc dichloride; the copper powder of described precipitate and separate is filtered, washs, and 135 ℃ ~ 150 ℃ oven dry obtained the copper powder product in 22 ~ 24 hours under protection of inert gas again.
2. the treatment process of the waste liquid after a printed circuit board (PCB) copper coating cleans, it is characterized in that: be that 99.9% zinc powder adds in the waste liquid after the printed circuit board (PCB) copper coating cleans and reacts with 65 ~ 80 orders, weight percentage, adding the zinc powder amount is that every liter of waste liquid adds 300g, temperature of reaction is 70 ~ 75 ℃, and the limit adds the induction stirring reaction of zinc powder limit and obtained liquor zinci chloridi and copper powder in 4 hours; Reacted solution was squeezed into settling pool heavy clear 24 hours; supernatant liquor zinc chloride and bottom copper powder precipitate and separate, supernatant liquor evaporative crystallization are obtained anhydrous zinc dichloride; the copper powder of described precipitate and separate is filtered, washs, and 135 ℃ of oven dry obtained the copper powder product in 22 hours under protection of inert gas again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104578055A CN102557297B (en) | 2011-12-31 | 2011-12-31 | Treatment method of waste liquid after cleaning copper plated layer of printed circuit board |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104578055A CN102557297B (en) | 2011-12-31 | 2011-12-31 | Treatment method of waste liquid after cleaning copper plated layer of printed circuit board |
Publications (2)
| Publication Number | Publication Date |
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| CN102557297A CN102557297A (en) | 2012-07-11 |
| CN102557297B true CN102557297B (en) | 2013-10-02 |
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| CN2011104578055A Expired - Fee Related CN102557297B (en) | 2011-12-31 | 2011-12-31 | Treatment method of waste liquid after cleaning copper plated layer of printed circuit board |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103480860B (en) * | 2013-09-25 | 2016-01-06 | 广东致卓精密金属科技有限公司 | Alkaline etching waste liquid for producing printed circuit board is utilized to prepare the method for high-purity nano copper |
| CN107522334A (en) * | 2016-12-28 | 2017-12-29 | 江西中信华电子工业有限公司 | A kind of copper powder filter used for printed circuit board |
| CN113526761B (en) * | 2021-05-26 | 2024-04-30 | 深圳世伦五金电子有限公司 | Method and system for treating surface coating cleaning waste liquid of electronic connector |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5279641A (en) * | 1992-08-25 | 1994-01-18 | Nikko Fine Products Co., Ltd. | Method for concurrent production of copper powder and a metal chloride |
| JP3002302B2 (en) * | 1991-07-25 | 2000-01-24 | キヤノン株式会社 | Data processing device |
| CN1534111A (en) * | 2003-03-28 | 2004-10-06 | 巫协森 | Method of recovering copper metal from waste printed circuit board and copper containing waste liquid and its device |
| CN101058436A (en) * | 2006-04-17 | 2007-10-24 | 上饶市华丰铜业有限公司 | Circuit board and electric plating sludge resource recovery process |
| CN101353795A (en) * | 2008-08-26 | 2009-01-28 | 湖南万容科技有限公司 | Method for extracting copper from printed circuit board acidic spent etching solution and preparing poly ferric chloride |
| CN101372037A (en) * | 2007-08-23 | 2009-02-25 | 高愈尊 | Method for preparing nano copper powder |
| CN101890506A (en) * | 2010-07-31 | 2010-11-24 | 太原理工大学 | Method for preparing nano-copper |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH032302A (en) * | 1989-05-26 | 1991-01-08 | Nisshin Steel Co Ltd | Manufacture of high purity copper fine powder |
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2011
- 2011-12-31 CN CN2011104578055A patent/CN102557297B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3002302B2 (en) * | 1991-07-25 | 2000-01-24 | キヤノン株式会社 | Data processing device |
| US5279641A (en) * | 1992-08-25 | 1994-01-18 | Nikko Fine Products Co., Ltd. | Method for concurrent production of copper powder and a metal chloride |
| CN1534111A (en) * | 2003-03-28 | 2004-10-06 | 巫协森 | Method of recovering copper metal from waste printed circuit board and copper containing waste liquid and its device |
| CN101058436A (en) * | 2006-04-17 | 2007-10-24 | 上饶市华丰铜业有限公司 | Circuit board and electric plating sludge resource recovery process |
| CN101372037A (en) * | 2007-08-23 | 2009-02-25 | 高愈尊 | Method for preparing nano copper powder |
| CN101353795A (en) * | 2008-08-26 | 2009-01-28 | 湖南万容科技有限公司 | Method for extracting copper from printed circuit board acidic spent etching solution and preparing poly ferric chloride |
| CN101890506A (en) * | 2010-07-31 | 2010-11-24 | 太原理工大学 | Method for preparing nano-copper |
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